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August 20, 2003Proceedings of the National Academy of Sciences2,854 citationsOpen Access

Increase in signal-to-noise ratio of > 10,000 times in liquid-state NMR

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JAJan Henrik Ardenkjær‐LarsenBFBjörn FridlundAGAndreas Gram

Key Points

  • To develop a method for creating strongly hyperpolarized nuclear spins in solution to dramatically increase liquid-state NMR sensitivity and reduce measurement time.
  • Polarized solid samples at low temperature in a 3.35 T superconducting magnet using dynamic nuclear polarization driven by ~94 GHz microwave irradiation.
  • Rapidly dissolved the solid sample with a solvent injection system inside the polarizer while preserving nuclear spin polarization.
  • Measured polarization retention and NMR signal enhancement using aqueous [13C]urea transferred to a high-resolution 9.4 T spectrometer.
  • Achieved post-dissolution liquid-state polarizations of 37% for 13C and 7.8% for 15N in [13C]urea.
  • Yielded signal enhancements of 44,400-fold for 13C and 23,500-fold for 15N compared with thermal equilibrium at room temperature and 9.4 T.

Abstract

A method for obtaining strongly polarized nuclear spins in solution has been developed. The method uses low temperature, high magnetic field, and dynamic nuclear polarization (DNP) to strongly polarize nuclear spins in the solid state. The solid sample is subsequently dissolved rapidly in a suitable solvent to create a solution of molecules with hyperpolarized nuclear spins. The polarization is performed in a DNP polarizer, consisting of a super-conducting magnet (3.35 T) and a liquid-helium cooled sample space. The sample is irradiated with microwaves at approximately 94 GHz. Subsequent to polarization, the sample is dissolved by an injection system inside the DNP magnet. The dissolution process effectively preserves the nuclear polarization. The resulting hyperpolarized liquid sample can be transferred to a high-resolution NMR spectrometer, where an enhanced NMR signal can be acquired, or it may be used as an agent for in vivo imaging or spectroscopy. In this article we describe the use of the method on aqueous solutions of 13Curea. Polarizations of 37% for 13C and 7.8% for 15N, respectively, were obtained after the dissolution. These polarizations correspond to an enhancement of 44,400 for 13C and 23,500 for 15N, respectively, compared with thermal equilibrium at 9.4 T and room temperature. The method can be used generally for signal enhancement and reduction of measurement time in liquid-state NMR and opens up for a variety of in vitro and in vivo applications of DNP-enhanced NMR.

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Cite This Study

Ardenkjær‐Larsen et al. (2003) studied this question.

synapsesocial.com/papers/69d73c123f2a6ac123b8ac3ehttps://doi.org/10.1073/pnas.1733835100
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